CN102675057B - A kind of catalytic distillation technology method of synthesizing methyl tertbutyl ether - Google Patents
A kind of catalytic distillation technology method of synthesizing methyl tertbutyl ether Download PDFInfo
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- CN102675057B CN102675057B CN201210051632.1A CN201210051632A CN102675057B CN 102675057 B CN102675057 B CN 102675057B CN 201210051632 A CN201210051632 A CN 201210051632A CN 102675057 B CN102675057 B CN 102675057B
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Abstract
The present invention is a kind of catalytic distillation technology method of synthesizing methyl tertbutyl ether.It is characterized in that catalytic distillation tower is divided into Shang Ta and Xia Ta of series connection, upper tower to be made up of rectifying section and conversion zone, lower tower is stripping section；Upper tower pressure is that Conventional catalytic distills synthesizing methyl tertbutyl ether pressure, and lower pressure tower is lower than upper tower pressure；Reboiler at the bottom of tower tower under the Topography of column overhead steam in utilization；Upper tower is provided with auxiliary condenser.It is characteristic of the invention that saving energy consumption, than Conventional catalytic distillation column energy-conservation more than 45%, product purity is high, and molar purity is up to 99.8%, and isobutene conversion reaches 99%.
Description
Technical field:
The present invention is a kind of catalytic distillation technology method of synthesizing methyl tertbutyl ether.Belong to high-purity methyl tertbutyl ether
Production.Specifically refer to a kind of new process utilizing differential pressure heat coupling and catalyzing distillation column to carry out methyl tertiary butyl ether(MTBE) synthesis.
Background technology:
Methyl tertiary butyl ether(MTBE) is called for short MTBE, is the excellent mediation component improving octane number, although the U.S. was in 2008
Disabling MTBE is as the octane enhancing additive of gasoline the most comprehensively, but owing to the Asia application MTBE time is later, various countries do not limit
Or the decree of disabling puts into effect, and the demand of gasoline quickly increases by developing Asia and Middle East various countries, and in gasoline
Benzene, aromatic hydrocarbons, sulfur and alkene have strict restriction, and therefore continuation is increased by MTBE demand.
Methyl tertiary butyl ether(MTBE) is again the important source material of high-purity isobutene., is also important solvent and reagent simultaneously.
The raw material of methyl tertiary butyl ether(MTBE) production technology is methanol and the C4 fraction containing isobutene..The C4 fraction of isobutene. has two kinds of sources,
A kind of C4 fraction coming from catalytic cracking unit, a kind of C4 after Butadiene Extraction being ethylene cracker and producing
Fraction.
Synthesizing methyl tertbutyl ether production technology is mainly etherification technology, according to the difference of methyltertiarvbutyl ether reactor, methyl-tert fourth
The following several forms of base ether synthetic technology existence: (1) fixed bed reaction technology；(2) expanded bed reaction technology；(3) expanded bed-urge
Change distillation reaction technology；(4) mixed phase reactive distillation technology；(5) catalytic distillation reaction technology.Combination with catalytic distillation as core
Technique has become as technological subject.
First United States Patent (USP) US4232177 proposes to be used for producing high-purity MTBE by catalytic distillation process.US4439350 sets
Count out tower internals structure, developed into catalytic distillation technology, can be used for producing high-purity MTBE.US4475005 designs
The reactive distillation column of another kind of tower internals prepares MTBE technology, the operation pressure 800KPa of tower, reflux ratio in embodiment
It is 1.US4504687 describes and prepares MTBE and the method for low content isobutene. C4 logistics.C4 logistics containing isobutene. and first
The reaction of alcohol is carried out in catalytic distillation tower, wherein reacts and distills and carries out at various pressures by structural measure.According to
Tower is divided into distillation fraction and reactive moieties by pressure.The catalytic distillation technology that US5118873 and US5120403 proposes is all distillation
Improvement in tower internal structure.
Sinopec (CN1042664A) has developed into another kind of catalytic distillation technology, designs novel device and urges
Agent loading method.Chinese patent CN1349964A prepares the method for high purity raffinute II and methyl tertiary butyl ether(MTBE).The method is divided
In two stages, the first stage, isobutene. and methanol reacted to balance formation MTBE, at second-order in one or more reactors
Section, in reactive distillation column, the isobutene. of mixture residual reacts on acidic catalyst.
European patent EP 0885866A1 discloses a kind of by the C4 hydrocarbon stream containing isobutene. and first with six embodiments
Alcohol reacts the method preparing MTBE.The common feature of all embodiments is at least one pre-reactor, a reactive distillation column
It is connected in series with a subsequent reactor.
The most simple catalytic distillation technology or catalytic distillation group technology, although catalytic distillation tower will reaction and steaming
Evaporate PROCESS COUPLING, it is achieved that the utilization of reaction heat, but, still suffer from the bottleneck that the thermodynamic efficiency of distillation column own is low, energy consumption is big,
Because the heat of reboiler is by being discharged by condenser after distillation column in above-mentioned distillation column, cause energy expenditure, thermodynamics
Efficiency is low.
Summary of the invention
The technical problem to be solved is to provide a kind of catalytic distillation technology method of synthesizing methyl tertbutyl ether,
It is the separation of the synthesis and product that utilize differential pressure heat coupling and catalyzing distillation column to realize methyl tertiary butyl ether(MTBE), by course of reaction,
Product separates organically to combine and carries out simultaneously, can directly obtain highly purified MTBE product, and be coupled by energy
Two different towers of pressure will be divided into by reactive distillation column, utilize high pressure overhead vapours as the thermal source at the bottom of lower pressure column, thus
Reach the purpose that still-process is the most energy-conservation.
The present invention solves that the synthesizer that its technical problem is used includes Shang Ta, Xia Ta, compressor, heat exchanger, auxiliary
Helping condenser and pump, be divided into rectifying section and conversion zone two parts inside upper tower, wherein rectifying section has 5-14 block theoretical plate, conversion zone
There is 7-16 block theoretical plate；Lower tower is stripping section, has 6-15 block theoretical plate.Tower spirit at lower column overhead gas phase delivery line Yu upper tower
Installing compressor between phase feed pipe, the tower bottom liquid of upper tower is directly entered lower tower mutually, feeds as lower column overhead, in upper column overhead
Product delivery line on be installed in series heat exchanger and auxiliary condenser, play condensation；Described pump is installed on auxiliary condenser
Outlet and upper column overhead return duct and unreacted C4 fraction product distillate between pipe.
The process utilizing said apparatus to carry out synthesizing methyl tertbutyl ether is: the reactant C4 fraction containing isobutene. is through pipe
Line enters bottom the conversion zone of upper tower, and reactant methanol fresh feed enters in the middle part of the conversion zone of upper tower through pipeline, so, and isobutyl
Alkene inversely contacts generation etherification reaction with methanol at conversion zone and generates methyl tertiary butyl ether(MTBE), and the methyl tertiary butyl ether(MTBE) generated passes through
Pipeline enters lower tower, and the tower reactor logistics part being left highly purified MTBE through the stripping effect of lower tower enters heat exchange through pipeline
Device, produces the steam that boils again and returns to tower reactor through pipeline, and another part is as lower tower tower reactor product bleeder.Upper tower conversion zone is the most anti-
The C4 fraction answered and methanol enter rectifying section, and the rectifying action through rectifying section obtains unreacted C4 fraction and methanol at tower top
And successively through pipeline, heat exchanger, pipeline and auxiliary condenser, the liquid phase part obtained after condensation is back to top of tower, one
Part is as upper top of tower product bleeder.Lower top of tower gas phase is entered from upper tower bottom through pipeline, compressor and pipeline successively
Enter conversion zone generation etherification reaction.
Under catalytic distillation tower of the present invention, the tower pressure of tower is 0.1-0.115MPa (absolute pressure), and upper tower pressure is for being conventionally synthesized MTBE
The pressure of catalytic distillation tower.In operating process, on differential pressure heat coupling and catalyzing distillation column, tower reflux ratio is 5-8, upper column overhead temperatures
For 60-90 DEG C, the temperature of upper tower conversion zone is 65-90 DEG C, and upper tower bottom temperature is 70-90 DEG C, and lower column overhead temperatures is-10-
45 DEG C, lower tower bottom temperature is 50-65 DEG C.Charging is liquid phase feeding, and temperature is 20-45 DEG C, and methanol charging is pure methanol, first
The mol ratio of the isobutene. in alcohol and the C4 fraction containing isobutene. is 1.02: between 1-1.1: 1.
The invention has the beneficial effects as follows and catalytic distillation technology and differential pressure heat coupling rectification technology are combined, form differential pressure
Thermal coupling catalytic distillation technology, and be applied in methyl tertiary butyl ether(MTBE) synthetic reaction.Methyl tertiary butyl ether(MTBE) at the bottom of lower tower tower rubs
You reach 99.8% at purity, and isobutene conversion reaches 99%, reaches same isobutene conversion and product purity requirement, than routine
Catalytic distillation flow process can save energy more than 45%, and this is that a course of reaction couples with separation process, go up simultaneously tower condenser with under
The technology of tower reboiler thermal coupling, is ensureing reaction conversion ratio and energy consumption can be greatly reduced the most simultaneously.
Fig. 1 is based on the catalytic distillation technology flow process of a kind of synthesizing methyl tertbutyl ether (MTBE) proposed by the invention and shows
It is intended to.
In figure, the upper tower of 1-, tower under 2-, 3-compressor, 4-heat exchanger, 5-auxiliary condenser, 6-pump, 7,8,9 ... 19-manages
Line.
Detailed description of the invention:
The invention will be further described with embodiment below in conjunction with the accompanying drawings, but the invention is not limited in embodiment.
Embodiment 1: flow process as shown in Figure 1, each Region Theory plate number is as shown in table 1, containing isobutene. C4 fraction charging group
Becoming as shown in table 2, methanol charging is 1.02: 1 with isobutene. mol ratio, methanol, C4 fraction containing isobutene. feed entrance point (from
On down count) to be followed successively by the 15th piece of theoretical plate of tower (1), the 20th piece of theoretical plate and methanol feeding temperature be 20 DEG C, containing isobutene.
The feeding temperature of C4 fraction be 45 DEG C.Upper tower (1) top of the differential pressure heat coupling and catalyzing distillation column of synthesizing methyl tertbutyl ether
Reflux ratio is 8, and each logistics flux and composition are as shown in table 3, and upper tower (1) top temperature is 68.2 DEG C, upper tower (1) still temperature 78.3 DEG C, on
Tower (1) conversion zone temperature is 71.4 DEG C-78.3 DEG C, and lower tower (2) top temperature is-2.1 DEG C, and lower tower (2) still temperature is 55.2 DEG C, upper tower
(1) operation pressure is 1MPa, and lower tower (2) operation pressure is 0.1MPa.Lower top of tower gas phase is compressed to by compressor (3)
1.09MPa, 80 DEG C, isobutene conversion reaches 99%, and the molar purity of lower tower (2) bottom product methyl tertiary butyl ether(MTBE) is
99.8%.Reaching same conversion ratio and product separation requirement, needed for this technological process, total energy consumption is 4924kW, and Conventional catalytic distills
Flow process total energy consumption is 13284kW, compares and can save energy 62.93%.
Table 1 embodiment 1 each Region Theory plate number
| Region | Upper tower rectifying section | Upper tower conversion zone | Lower tower |
| Number of theoretical plate | 10 | 10 | 10 |
Table 2 embodiment 1 C4 fractional composition Han isobutene.
| Component | Mass fraction/% |
| Propane | 0.411 |
| Iso-butane | 54.912 |
| Isobutene. | 41.848 |
| Normal butane | 1.626 |
| 1-butylene | 0.401 |
| Cis-2-butene | 0.401 |
| Trans-2-butene | 0.401 |
The each logistics quality flow of table 3 embodiment 1 and each constituent mass mark
Embodiment 2: flow process as shown in Figure 1, each Region Theory plate number is as shown in table 4, containing isobutene. C4 fraction charging group
Becoming as shown in table 2, methanol charging is 1.1: 1 with isobutene. mol ratio, methanol, C4 fraction containing isobutene. feed entrance point (from
On down count) be followed successively by the 10th piece of theoretical plate of tower (1), the 12nd piece of theoretical plate is 25 DEG C with methanol feeding temperature, containing isobutene.
The feeding temperature of C4 fraction be 40 DEG C.Upper tower (1) top of the differential pressure heat coupling and catalyzing distillation column of synthesizing methyl tertbutyl ether
Reflux ratio is 5, and each logistics flux and composition are as shown in table 5, and upper tower (1) top temperature is 67 DEG C, upper tower bottom temperature 82.4 DEG C, upper tower
Conversion zone temperature 71-82.5 DEG C, lower tower (2) tower top temperature 16.3 DEG C, lower tower (2) still temperature is 57.4 DEG C, upper tower (1) operation pressure
For 1MPa, lower tower (2) operation pressure is 0.11MPa.Lower top of tower gas phase is compressed to 1.08MPa by compressor (3), 93 DEG C, different
Butene conversion reaches 99.38%, and the molar purity of lower tower (2) bottom product methyl tertiary butyl ether(MTBE) is 99.8%.Reach same
Conversion ratio and product separation requirement, needed for this technological process, total energy consumption is 3265kW, and Conventional catalytic distillation flow process total energy consumption is
9718kW, compares and can save energy 66.4%.
Table 4 embodiment 2 each Region Theory plate number
| Region | Upper tower rectifying section | Upper tower conversion zone | Lower tower |
| Number of theoretical plate | 5 | 7 | 6 |
The each logistics quality flow of table 5 embodiment 2 and each constituent mass mark
Embodiment 3: flow process as shown in Figure 1, each Region Theory plate number is as shown in table 6, containing isobutene. C4 fraction charging group
Becoming as shown in table 2, methanol charging is 1.06: 1 with isobutene. mol ratio, methanol, C4 fraction containing isobutene. feed entrance point (from
On down count) be followed successively by the 21st piece of theoretical plate of tower (1), the 30th piece of theoretical plate is 20 DEG C with methanol feeding temperature, containing isobutene.
The feeding temperature of C4 fraction be 45 DEG C.Upper tower (1) top of the differential pressure heat coupling and catalyzing distillation column of synthesizing methyl tertbutyl ether
Reflux ratio is 6.5, and each logistics flux and composition are as shown in table 7, and upper tower (1) top temperature is 67.5 DEG C, upper tower (1) still temperature 81 DEG C, on
Tower (1) conversion zone temperature is 71 DEG C-81 DEG C, and lower tower (2) top temperature is 45 DEG C, and lower tower (2) still temperature is 59 DEG C, upper tower (1) operation pressure
Power is 1MPa, and lower tower (2) operation pressure is 0.115MPa.Lower top of tower gas phase is compressed to 1.19MPa by compressor (3), and 130
DEG C, isobutene conversion reaches 99.17%, and the molar purity of lower tower (2) bottom product methyl tertiary butyl ether(MTBE) is 99.99%.Reach
To same conversion ratio and product separation requirement, needed for this technological process, total energy consumption is 6013kW, Conventional catalytic distillation flow process total energy
Consumption is 11575kW, compares and can save energy 48%.
Table 6 embodiment 2 each Region Theory plate number
| Region | Upper tower rectifying section | Upper tower conversion zone | Lower tower |
| Number of theoretical plate | 14 | 16 | 15 |
The each logistics quality flow of table 7 embodiment 2 and each constituent mass mark
When be can be seen that differential pressure heat coupled reaction rectifying column technology is applied to methyl acetate synthetic reaction by above-described embodiment, under
At the bottom of tower tower, methyl tertiary butyl ether(MTBE) molar purity reaches more than 99.8%, and isobutene conversion, more than 99%, reaches same isobutene.
Conversion ratio and product separation requirement, can save energy more than 45% than Conventional catalytic distillation flow process, and this is a course of reaction and separate
PROCESS COUPLING, goes up the technology of tower condenser and lower tower reboiler thermal coupling simultaneously, is ensureing that reaction conversion ratio is same with selective
Time energy consumption can be greatly reduced.
Claims (4)
1. the catalytic distillation technology method of a synthesizing methyl tertbutyl ether, it is characterised in that:
A. with the C4 fraction containing isobutene. and methanol for raw material synthesizing methyl tertbutyl ether in catalytic distillation tower, catalytic distillation tower
Being divided into Shang Ta and Xia Ta, upper tower to be made up of rectifying section and conversion zone, lower tower is stripping section；
B. go up tower operation pressure for being conventionally synthesized methyl tertiary butyl ether(MTBE) catalytic distillation pressure tower, lower tower operation pressure ratio on tower operate
Pressure is low；
C. the reboiler at the bottom of tower tower under the Topography of upper column overhead steam is utilized；
D. descend column overhead gas phase from entering upper tower at the bottom of upper tower tower after compressor compresses；
E. go up tower tower bottom liquid and enter lower tower directly from lower column overhead；
Wherein, the C4 fraction autoreaction pars infrasegmentalis containing isobutene. described in a enters upper tower, enters in the middle part of methanol autoreaction section
Tower, the isobutene. in C4 fraction reacts with methanol conversion zone in upper tower, and the methyl tertiary butyl ether(MTBE) of generation is from the bottom of lower tower
Portion flows out, and unreacted C 4 fraction and methanol are from upper top of tower extraction；
Upper column overhead temperatures described in a is 60-90 DEG C, and upper tower conversion zone temperature is 65-90 DEG C, and upper tower bottom temperature is 70-
90 DEG C, lower column overhead temperatures is-10-45 DEG C, and lower tower bottom temperature is 50-65 DEG C；
Methanol described in a is 1.02: 1-1.1: 1 with the mol ratio of the isobutene. in the C4 fraction containing isobutene..
The catalytic distillation technology method of a kind of synthesizing methyl tertbutyl ether the most according to claim 1, it is characterised in that described in b
The operation pressure of lower tower be 0.1-0.115MPa absolute pressure.
The catalytic distillation technology method of a kind of synthesizing methyl tertbutyl ether the most according to claim 1, it is characterised in that described in c
Upper tower auxiliary condenser is set.
The catalytic distillation technology method of a kind of synthesizing methyl tertbutyl ether the most according to claim 1, it is characterised in that described in d
Lower column overhead gas phase be compressed to upper tower tower reactor pressure or higher than upper tower tower reactor pressure through compressor, temperature supreme tower bottom temperature
Or higher than upper tower bottom temperature, then from entering tower at the bottom of Shang Tata.
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| CN201210051632.1A CN102675057B (en) | 2012-02-25 | 2012-02-25 | A kind of catalytic distillation technology method of synthesizing methyl tertbutyl ether |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104803832B (en) * | 2015-03-23 | 2017-03-22 | 中国神华能源股份有限公司 | MTBE (methyl tert-butyl ether) production system |
| CN109851485B (en) * | 2019-01-28 | 2020-04-28 | 重庆大学 | Method and system for producing 2-methoxy-2-methylheptane by differential pressure thermal coupling reaction rectification |
| CN114177853A (en) * | 2021-10-29 | 2022-03-15 | 武汉金中石化工程有限公司 | MTBE device |
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| CN1050828A (en) * | 1990-12-03 | 1991-04-24 | 中国石油化工总公司 | Mixed phase catalysis reaction distillation technology and equipment |
| EP0470655A1 (en) * | 1990-08-01 | 1992-02-12 | ENIRICERCHE S.p.A. | Process for preparing tertiary alkyl ethers and apparatus for reactive distillation |
| WO1996001244A1 (en) * | 1994-07-01 | 1996-01-18 | Neste Oy | Process and apparatus for preparing tertiary alkyl ethers |
| CN101381287A (en) * | 2008-10-18 | 2009-03-11 | 岳阳桦科化工有限责任公司 | Method for producing MTBE from four-carbon compounds and methanol |
-
2012
- 2012-02-25 CN CN201210051632.1A patent/CN102675057B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0470655A1 (en) * | 1990-08-01 | 1992-02-12 | ENIRICERCHE S.p.A. | Process for preparing tertiary alkyl ethers and apparatus for reactive distillation |
| CN1050828A (en) * | 1990-12-03 | 1991-04-24 | 中国石油化工总公司 | Mixed phase catalysis reaction distillation technology and equipment |
| WO1996001244A1 (en) * | 1994-07-01 | 1996-01-18 | Neste Oy | Process and apparatus for preparing tertiary alkyl ethers |
| CN101381287A (en) * | 2008-10-18 | 2009-03-11 | 岳阳桦科化工有限责任公司 | Method for producing MTBE from four-carbon compounds and methanol |
Non-Patent Citations (3)
| Title |
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| 16万吨/年MTBE装置催化精馏塔的建模与控制仿真;李静;《中国优秀硕士学位论文全文数据库（电子期刊）工程科技Ⅰ辑》;20101229;第7-8页 * |
| 反应精馏塔应用于差压热耦合精馏技术的模拟;孙兰义 等;《化工进展》;20111115;第30卷;149-153 * |
| 反应精馏应用于内部热耦合精馏以及差压热耦合精馏技术的模拟研究;宁亚南;《中国优秀硕士学位论文全文数据库（电子期刊）工程科技Ⅰ辑》;20110501;50-69 * |
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